Performance in (Ultra‐)high‐performance liquid chromatography—How to qualify and optimize instruments in practice

Jaekel, Alexander; Wirtz, Michaela; Lamotte, Stefan; Legelli, Mo

doi:10.1002/jssc.202200894

Cited by 5 publications

(6 citation statements)

References 39 publications

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“…It is important for mass instrument, that the mobile phase flow rate does not exceed 0.5 mL/min in the analysis performed in mass detectors based on liquid chromatography [23]. Therefore, the analysis conditions had to be changed, and the mobile phase flow rate was reduced to 0.5 mL/min throughout the high-resolution mass spectrometric analyses [24,25]. The gradient mode has been redesigned as follows: zeroth min 35% mobile phase A; 0.0−8.00 min gradient up to 90% mobile phase A; 8.01−10.0 min gradient continued 90% mobile phase A; 10.00−10.01 min gradient down to 35% mobile phase A; 10.01−12.00 min gradient continued 35% mobile phase A to condition the stationary phase to initial conditions.…”

Section: Lcms-it-tof Methods Developmentmentioning

confidence: 99%

Liquid chromatographic determination of lumacaftor in the presence of ivacaftor and identification of five novel degradation products using high‐performance liquid chromatography ion trap time‐of‐flight mass spectrometry

Özcan,

Erdoğan Uzunoğlu,

Levent

et al. 2023

J of Separation Science

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Lumacaftor is a transmembrane conductance regulator potentiator drug, prescribed for the treatment of cystic fibrosis in patients who are homozygous for the F508del mutation. Quantitation of lumacaftor besides its degradation products and ivacaftor was achieved on a fused-core silica particle column packed with pentafluorophenylpropyl stationary phase (Ascentis Express F5, 2.7 μm particle size 100 mm × 4.6 mm; Supelco) using gradient elution (A: 0.1% [v/v] formic acid in water, B: 0.1% [v/v] formic acid in acetonitrile [the mobile phase pH 2.5]). A constant flow rate at 1 mL/min was applied, and the detection was realized using a photodiode array detector set at 216 nm. The pseudo tablet formulation of the lumacaftor/ivacaftor fixed-dose combination preparation, namely, Orkambi R , was prepared in vitro and used for the analytical performance validation and method application studies. In addition, five novel degradation products, four of which even have no Chemical Abstracts Services registry number, were identified using high-resolution mass spectrometry instrument, and their possible mechanisms of formation were proposed. According to current literature, this paper can be regarded as the most comprehensive liquid chromatographic study on lumacaftor determination, among its counterparts.

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Section: Lcms-it-tof Methods Developmentmentioning

confidence: 99%

Liquid chromatographic determination of lumacaftor in the presence of ivacaftor and identification of five novel degradation products using high‐performance liquid chromatography ion trap time‐of‐flight mass spectrometry

Özcan,

Erdoğan Uzunoğlu,

Levent

et al. 2023

J of Separation Science

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“…Although we know many functions of the compounds in WDT, few can be identified in the cerebrospinal fluid (CSF). Ultra-high-performance liquid chromatography (UHPLC)-high-resolution mass spectrometry (HRMS) is an important tool for efficiently separating and identifying different components in fluid samples [13][14]. We obtained CSF metabolites affected by WDT using UHPLC-HRMS.…”

Section: Introductionmentioning

confidence: 99%

Analysis of cerebrospinal fluid metabolites affected by WenDanTang based on ultra‐high‐performance liquid chromatography coupled with high‐resolution mass spectrometry

Zou,

Tang,

et al. 2024

J of Separation Science

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WenDanTang (WDT) is a Chinese herbal formula used to treat various diseases, including neurodegenerative diseases. However, the neuroprotective metabolic pathways and the components involved in this process are not fully understood. In this study, we examined the neuroprotective metabolic pathways of WDT in rat brains using cerebrospinal fluid metabolomics and ultra‐high‐performance liquid chromatography–high‐resolution mass spectrometry. Twelve rats were randomly divided into a WDT (administrated with WDT solution) and a control group. The ultra‐high‐performance liquid chromatography technique was used to explore the components of the WDT solution and cerebrospinal fluid, and secondary mass spectra of cerebrospinal fluid were used to identify possible brain‐incorporating components after WDT. The results of the differential metabolism analysis showed that eight metabolites were typically altered (all p < 0.05). By comparing the secondary mass spectra of the cerebrospinal fluid of rats and WDT solution, two possible brain‐incorporating components of WDT, stachydrine and α‐methoxyphenylacetic acid, were identified. The data also suggested that WDT affects nucleotide metabolism, glutathione metabolism, and B‐vitamin metabolic pathways, the central differential metabolic pathways. These data suggest that WDT protects neurons through its active components, such as stachydrine, and regulates biochemical metabolism to affect the brain's energy metabolism and antioxidant capacity.

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“…These are the needle seat capillary, the connection tubing between the injector valve and the column compartment, and the heat exchanger capillary. While extra-column band broadening from all or part of them could be decreased somewhat by using smaller-id or shorter-length capillaries, 20 they are limited by practical aspects, such as ease of handling and pressure drop concerns.…”

Section: ■ Introductionmentioning

confidence: 99%

Minimize Precolumn Band Broadening with Immiscible Solvent Sandwich Injection

Zhu,

Pursch,

Huygens

et al. 2023

Anal. Chem.

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We investigated the possibility of reducing the effect of precolumn band broadening (PreCBB) by sandwiching the sample between two small plugs of an immiscible liquid. It has been found that in cases of severe PreCBB, improvements in peak efficiency can amount up to 20 times for the early-eluting compounds. For smaller degrees of PreCBB, the gain on the efficiency of early-eluting compounds is smaller (order of 50%), yet it is still significant. It has been verified that the presence of the immiscible fluid sandwich does not affect the repeatability of the analysis nor the linearity of the calibration curves used for analyte quantitation. It is also shown that the main effect of the two sandwich plugs is the minimization of the dispersion in the precolumn transfer tubing itself, which makes the method fundamentally different from pure on-column focusing methods such as the performance optimizing injection sequence (POISe) method. It is further demonstrated that both halves of the sandwich are needed, since the beneficial effect is clearly much smaller when only one plug is present. A drawback of the method is that some of the late-eluting peaks are slightly adversely affected by the presence of the sandwich liquid in the case where 127 μm i.d. tubing was used. The mechanism for this peak deterioration effect is at present still unclear but only occurs under gradient conditions and is clearly linked to the size of the sandwich plugs (the smaller the plugs, the smaller the adverse effect) and the internal diameter of the tubing used between the injection valve and the column.

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Performance in (Ultra‐)high‐performance liquid chromatography—How to qualify and optimize instruments in practice

Cited by 5 publications

References 39 publications

Liquid chromatographic determination of lumacaftor in the presence of ivacaftor and identification of five novel degradation products using high‐performance liquid chromatography ion trap time‐of‐flight mass spectrometry

Liquid chromatographic determination of lumacaftor in the presence of ivacaftor and identification of five novel degradation products using high‐performance liquid chromatography ion trap time‐of‐flight mass spectrometry

Analysis of cerebrospinal fluid metabolites affected by WenDanTang based on ultra‐high‐performance liquid chromatography coupled with high‐resolution mass spectrometry

Minimize Precolumn Band Broadening with Immiscible Solvent Sandwich Injection

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